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Commission Regulation (EEC) No 2568/91 of 11 July 1991 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis
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Article 1.(1) Oils, the characteristics of which comply with those set...
Article 2.(1) The characteristics of oils laid down in Annex I...
Article 2a.(1) For the purpose of this Article, ‘ olive oil...
Article 3.Where it is found that an oil does not correspond...
Article 4.(1) The Member States may approve assessment panels so that...
Article 6.(1) The oil content of oil cake and other residues...
Article 7.The Community provisions concerning the presence of contaminants shall apply....
Article 7a.Natural or legal persons and groups of persons who hold...
Article 8.(1) Member States shall notify the Commission of the measures...
Article 10.(1) This Regulation shall enter into force on the third...
SAMPLING OF OLIVE OIL OR OLIVE-POMACE OIL DELIVERED IN IMMEDIATE PACKAGING
DECISION TREE FOR VERIFYING WHETHER AN OLIVE OIL SAMPLE IS CONSISTENT WITH THE CATEGORY DECLARED
DETERMINATION OF PEROXIDE VALUE
5.1. Chloroform, analytical reagent quality, freed from oxygen by bubbling a...
5.2. Glacial acetic acid, analytical reagent quality, freed from oxygen by...
5.3. Potassium iodide, saturated aqueous solution, recently prepared, free from iodine...
5.4. Sodium thiosulphate, 0,01 mol/l (equivalent to 0,01 N) accurately standardised...
5.5. Starch solution, 10 g/l aqueous dispersion, recently prepared from natural...
DETERMINATION OF WAX CONTENT BY CAPILLARY COLUMN GAS CHROMATOGRAPHY
3.2. Glass column for gas chromatography, internal diameter 15,0 mm, length...
3.3. Suitable gas chromatograph with a capillary column, equipped with a...
3.4. 10 μl microsyringe for on-column injection, equipped with a hardened...
3.8. Analytical balance with guaranteed precision of ± 0,1 mg.
4.2. Potassium hydroxide ethanolic solution, approximately 2 N.
4.4. Potassium hydroxide ethanolic solution, approximately 0,2 N.
4.6. Glass plates (20x20 cm) coated with silica gel, without fluorescence...
4.14. 2,7-dichlorofluorescein, 0,2 % in ethanolic solution. Make slightly basic by...
4.15. Anhydrous pyridine, for chromatography quality (see Note 5).
4.19. α-cholestanol, purity more than 99 % (purity must be checked...
4.20. α-cholestanol internal standard solution, 0,2 % solution (m/V) in ethyl...
4.21. Phenolphthalein solution, 10 g/L in ethanol (point 4.10).
4.22. Carrier gas: hydrogen or helium, gas-chromatographic purity.
4.23. Auxiliary gases: hydrogen, helium, nitrogen and air, of gas-chromatographic purity....
4.24. n-Hexane (point 4.9)/ethyl ether (point 4.10) mixture 65:35 (V/V).
4.25. Silylation reagent, consisting of a 9:3:1 (V/V/V) mixture of pyridine/hexamethyl...
5.1. Preparation of the unsaponifiable matter.
5.1.1. Using a 500 μl microsyringe (point 3.6) introduce into the...
5.1.2. Add 50 ml of 2 N ethanolic potassium hydroxide solution...
5.1.3. Transfer the contents of the flask quantitatively into a 500...
5.1.4. Combine the three ether extracts in one separating funnel containing...
5.1.5. Evaporate the solvent by distillation on a rotary evaporator at...
5.2. Separation of the sterol and triterpene dialcohols fraction (erythrodiol +...
5.2.1. Preparation of the basic thin layer chromatography plates. Immerse the...
5.2.2. Place hexane/ethyl ether mixture (point 4.24) (Note 4) into the...
5.2.3. Prepare an approximately 5 % solution of the unsaponifiable (point...
5.2.4. Place the plate in the developing chamber prepared as specified...
5.2.5. Spray the plate lightly and uniformly with the 2,7-dichlorofluorescein solution...
5.2.6. By using a metal spatula, scrape off the silica gel...
DETERMINATION OF ERYTHRODIOL AND UVAOL
DETERMINATION OF THE PERCENTAGE OF 2-GLYCERYL MONOPALMITATE
3.3. Glass chromatograph column, internal diameter 21-23 mm, length 400 mm,...
3.7. 10 ml conical-bottomed centrifuge tubes with groundglass stopper
3.9. Thermostat permitting a stable temperature of 40 ± 0,5 °C...
3.14. Capillary gas chromatograph with an on-column cold injector for direct...
3.15. On-column cold injector for direct injection of the sample into...
3.17. Recorder-integrator adapted to the electrometer with a response rate no...
3.18. Capillary column made of glass or fused silica 8-12 metres...
3.19. 10 μl microsyringe fitted with a hardened needle, at least...
4.5. Pancreatic lipase. It must have an activity of between 2,0...
4.6. Buffer solution of trishydroxymethylaminomethane: 1 M aqueous solution adjusted to...
4.7. Enzyme-quality sodium cholate, 0,1 % aqueous solution (this solution must...
4.10. Developer solvent: mixture of n-hexane/diethyl ether (87:13 v:v)
4.13. Carrier gas: hydrogen or helium, for gas chromatography
4.14. Auxiliary gases: hydrogen, 99 % minimum purity, free from moisture...
4.16. Reference samples: pure monoglycerides or monoglyceride mixtures with a known...
DETERMINATION OF TRILINOLEIN CONTENT
DETERMINATION OF FATTY ACID METHYL ESTERS BY GAS CHROMATOGRAPHY
PART A PREPARATION OF THE FATTY ACID METHYL ESTERS FROM OLIVE OIL...
3.1. Trans-esterification with methanolic solution of potassium hydroxide at room temperature...
3.1.2.1. Methanol containing not more than 0,5 % (m/m) water.
3.1.2.6. Elution solvent for purifying the oil by column/SPE chromatography, mixture...
3.1.2.7. Potassium hydroxide, approximately 2M methanolic solution: dissolve 11,2 g of...
3.1.2.8. Silica gel cartridges, 1 g (6 ml), for solid phase...
PART B ANALYSIS OF FATTY ACID METHYL ESTERS BY GAS CHROMATOGRAPHY
DETERMINATION OF VOLATILE HALOGENATED SOLVENTS CONTENT OF OLIVE OIL
THE INTERNATIONAL OLIVE COUNCIL’S METHOD FOR THE ORGANOLEPTIC ASSESSMENT OF VIRGIN OLIVE OIL
9. PROCEDURE FOR THE ORGANOLEPTIC ASSESSMENT AND CLASSIFICATION OF VIRGIN OLIVE...
Method for calculating the median and the confidence intervals
(1) Wilkinson, L. 1990. Systat: The system for statistics. Evanston, IL.SYSTAT...
(2) Cicchitelli, G. 1984. Probabilità e Statistica. Maggioli Editore, Rimini.
(3) Massart, D.L.; Vandeginste, B.G.M.; Deming, Y.; Michotte, L. 1988. Chemometrics....
(4) Kendall, M.G.; Stuart, A. 1967. The advanced theory of statistics....
(5) McGill, R.; Tukey, J.W.; Larsen, W.A. 1978. Variation of Box...
(6) IOC/T.28/Doc. No 1 September 2007, Guidelines for the accreditation of...
NEUTRALIZATION AND DECOLORIZATION OF OLIVE OIL IN THE LABORATORY
ADDITIONAL NOTES 2, 3 AND 4 TO CHAPTER 15 OF THE COMBINED NOMENCLATURE
4.1. water, complying with the requirements of ISO 3696, Grade 3....
4.2. potassium iodide, 100 g/l solution, not containing iodate or free...
4.4. sodium thiosulfate, standard volumetric solution c (Na2S2O3.5H2O) = 0,1 mol/l,...
4.5. solvent, prepared by mixing equal volumes of cyclohexane and acetic...
4.6. Wijs reagent, containing iodine monochloride in acetic acid. Commercially available...
METHOD FOR THE DETERMINATION OF STIGMASTADIENES IN VEGETABLE OILS
4.1. 250 ml flasks suitable for use with a reflux condenser....
4.5. Glass chromatography column (1,5 to 2,0 cm internal diameter by...
4.6. Gas chromatograph with flame ionization detector, split or cold on-column...
4.7. Fused silica capillary column for gas chromatography (0,25 or 0,32...
4.8. Integrator-recorder with possibility of valley-valley integration mode.
4.9. 5 to 10 ml microsyringe for gas chromatography with cemented...
5.4. Alcoholic potassium hydroxide solution at 10 %. Add 10 ml...
5.5. Silica gel 60 for column chromatography, 70 to 230 mesh,...
5.6. Stock solution (200 ppm) of cholesta-3,5-diene (Sigma, 99 % purity)...
5.7. Standard solution of cholesta-3,5-diene hexane at concentration of 20 ppm,...
5.8. Solution of n-nonacosane in hexane at concentration of approximately 100...
5.9. Carrier gas for chromatography: helium or hydrogen of 99,9990 %...
5.10. Auxiliary gases for flame ionization detector: hydrogen of 99,9990 %...
Gas chromatogram obtained from a refined olive oil sample analysed...
4.1.3. Glass chromatographic column, 21 mm internal diameter, 450 mm length,...
4.1.4. Separating funnels, 250 ml, with normalised cone (male) at the...
4.1.12. Detector: differential refractometer. The full scale sensitivity should be at...
4.1.13. Column: stainless steel tube 250 mm length x 4,5 mm...
4.1.15. Vials, of about 2 ml volumes, with Teflon-layered septa and...
4.2.1. Petroleum ether 40– 60 °C chromatographic grade or hexane.
4.2.3. Elution solvent for purifying the oil by column chromatography mixture...
4.2.4. Silica gel, 70-230 mesh, type Merck 7734, with water content...
4.2.8. HPLC elution solvent: acetonitrile + acetone (proportions to be adjusted...
4.2.11. Solid phase extraction column with silica phase 1 g, 6...
4.5. Calculation of triacylglycerols composition (moles %) from fatty acid composition...
6. EXAMPLE (THE NUMBERS REFER TO THE SECTIONS IN THE TEXT...
DETERMINATION OF ALIPHATIC AND TRITERPENIC ALCOHOLS CONTENT BY CAPILLARY GAS CHROMATOGRAPHY
3.1. 250 ml round-bottomed flask fitted with a reflux condenser having...
3.4. Chromatographic tank for thin-layer chromatographic analysis, for glass plates of...
3.5. Ultraviolet lamp having a wavelength of 366 or 254 nm....
3.7. A cylindrical filter funnel with a G3 porous septum (porosity...
3.8. 50 ml vacuum conical flask with a 12/21 ground-glass female...
3.10. Gas chromatograph for use with a capillary column, and provided...
3.11. Glass or fused silica capillary column, of length 20 to...
3.12. Microsyringe for gas chromatography, of 10 μl capacity with hardened...
3.13. Analytical balance sensitive to 1 mg (with 0,1 mg display)....
4.1. Potassium hydroxide, approximately 2 N ethanolic solution: 130 g potassium...
4.4. Glass plates coated with silica gel, without fluorescence indicator, thickness...
4.5. Potassium hydroxide, approximately 0,2 N ethanolic solution; 13 g of...
4.11. Reference solution for thin-layer chromatography: C 20 -C 28 alcohols...
4.12. 0,2 % solution of 2', 7'-dichlorofluorescein in ethanol. Make slightly...
4.16. Standard solutions of trimethylsilyl ethers of aliphatic alcohols from C...
4.17. A 0,1 % (m/v) solution of 1-eicosanol in chloroform (internal...
4.18. Carrier gas: hydrogen or helium, gas-chromatographic purity.
5.2. Separation of alcoholic fractions
5.2.1. Preparation of basic TLC plates: the silica gel plates (4.4)...
5.2.2. Place a 65/35 by volume hexane/ethyl ether mixture in the...
5.2.3. An approximately 5 % solution of unsaponifiable matter (5.1.5) in...
5.2.4. Place the plate inside the development tank as stated in...
5.2.5. The plate is sprayed lightly and evenly with the solution...
5.2.6. Using a metal spatula scrape off the silica gel in...
5.4. Gas chromatography analysis
3.2. Glass column for liquid chromatography, internal diameter 15 mm, length...
3.3. Gas chromatograph suitable for use with a capillary column, equipped...
3.4. Microsyringe , 10 μl, with hardened needle, for direct on-column...
3.8. Analytical balance for weighing to an accuracy of ± 0,1...
METHOD FOR THE DETECTION OF EXTRANEOUS OILS IN OLIVE OILS
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